CHE 307-2

(Distillation)

1. 2. 5213189 3. 4. 5. 5213322

5213187

5213215

5213312

2554

CHE 307-2

(Distillation)

1. 2. 5213189 3. 4. 5. 5213322

5213187

5213215

5213312

2554

 1 1

1 1.1

1 1.2 1.3 1 1.4 1 2 2 2.1 2

2.2 4 2.2.1 4 2.2.2 , 5 3 6 3.1 3.1.1 -

6 6

3.1.2 6

3.2 7

4 8 4.1 4.2 5 15 5.1

8 9

5.2 6

15

16 . - 17

. - Refractometer 18 . T-xy and xy Diagram of Water and Ethanol at 1 atm 21 22

(Distillation) 5213187

1.

2.

5213189

3. 4. 5. : : 2554

5213215

5213312 5213322

60% ,80% , 90% Diagram

o

95%

95%

Equilibrium Still

65 o c

Dilute

Liquid Phase

Vapor Phase Refractometer Calibration

Vapor Phase Mol. Fraction; Y

Liquid Phase Mol. Fraction; T-xy

Constant Pressure Vapor Liquid Equilibrium 95%

mole Fraction of Liquid of Ethanol 95% 0.425 2

 90%

%brix

95% %brix

dilute ethanol vapor phase

vapor phase ethanol %brix

liquid phase

%brix phase ethanol

liquid phase vapor dilute ethanol 1 azeotrope azeotrope

4-1 ethanol 4-2 8

% Brix 8

Calibration Curve

2.1 Constant pressure vapor liquid equilibria 3 2.2 Minimum-boiling azeotropism in the system carbon disulfideacetone 3

3.1 The vapor-liquid equilibrium still 6 4.1 10 4.2 Constant pressure vapor liquid equilibrium 10 4.3 T-X,Y Diagram 11 4.4 Constant pressure vapor liquid equilibrium ( 11 4.5 T-X,Y Diagram ( 12 4.6 Constant pressure vapor liquid equilibrium ( 12 4.7 T-X,Y Diagram ( 13 4.8
( ) )

%Brix

dilute)

dilute)

Constant pressure vapor liquid equilibrium

dilute)

13

4.9 T-X,Y Diagram ( 14 .1 19

dilute)

Refractometer

.1 Constant pressure vapor liquid equilibria of water and ethanol at 1atm 21

.2 T-xy diagram of water and ethanol at 1 atm 21

1 1.1

1.2 1.2.1 1.2.2 -

1.2.3

T-X,Y diagram

1.3 1.3.1 1.3.2 ethanol

1.4 1.4.1

1.4.2 1.4.3 \ T-X,Y diagram

2.

2.1

(Phase rule)

F=C F C P Degree of freedom

P+2 (degree of freedom)

2 2 F=2 2+2=2

ethanol)

Degree of freedom

1 1 1 vapor phase(y1) liquid 4.1(a) vapor phase liquid

phase(x1) dew point curve bubble point curve

phase dew point curve saturated liquid

bubble point curve BC tie line B C saturated vapor tie line two phase mixture 4.1(a) 4.1(b) xy diagram 4.1(a) (Raoult s law) 4.2

4.2 liquid phase azeotrope azeotrope

acetone

carbon disulfide vapor phase

(a)

(b)

2.1 Constant pressure vapor liquid equilibria

2.2 Minimum-boiling azeotropism in the system carbon disulfideacetone

2.2 2.2.1

, 1,21,41,498, 110 122 -

1,4UNIQUAC Wilson 1,2-

UNIQUAC

Wilson

UNIQUAC

Wilson

2.2.2

+ + ,

, + -

+ (PVT) 148.8, 158.6, 168.5 2370 178.4

+ (Ruska)

k(,ij) k(,ij) k(,ij) k(,ij) k(,ij) 0.0312, 0.018, 0.0227 0.0232 ,

 3 3.1 3.1.1 1. Ethanol 95% 3.1.2 1. 2. 3. 4. 5. 6. equilibrium boiling vapor phase chamber boiling chamber receiver condensate still chamber boiling 400 ml 100 ml 2 8 4 2

3-1 The vapor-liquid equilibrium still

3.2

ethanol95% ethanol volume 60% 250 ml 60% ,

1. 80% , 90% , 2. 3. 4. heater % 5. 6.

boiling chamber condenser column heater

peristaltic pump heater boiling chamber

15 valve ( valve Q (

heater x) y) 65oC O

7. valve

8. 1 9.

2-7

equilibrium still

10. %Brix

Refractometer

4 4.1 % Brix ethanol Conc. ( % ) 0 10 20 % Brix 0 3.2 7 Conc. ( % ) 60 70 80 % Brix 17.5 18.7 19.1 Calibration Curve

4-1

30 40 50 Conc. (%) 60 80 90 95 4-2 Heater (% ) 40 40 40 40

10.3 14 16

90 100

19.2 17

Temp. ( oC ) 79 77 76 76

% Brix Liquid phase 16 18.1 18.8 19

dilute Vapor phase 16.7 17.5 18.4 18.4

% Brix Liquid phase 5.4 8.1 8.1 10.5

dilute Vapor phase 7.8 7.4 8.1 10.5

Conc. (%) 60 80 90 95

Concentration dilute Vapor Liquid phase phase 67.5 48 63 70.5 70.5 70.5 88.5 88.5

Concentration dilute Vapor Liquid phase phase 22.5 16 21 23.5 23.5 23.5 29.5 29.5

Vapor Liquid Phase Phase Mol.Frac, Mol.Frac Y ,X 0.413 0.238 0.365 0.447 0.447 0.447 0.722 0.722

4.2

ethanol

60%, 80%, 90%

95%

equilibrium still vapor mole

phase liquid phase %brix fraction of vapor phase mole fraction of liquid phase calibration curve mole fraction constant pressure vapor liquid equilibrium 4.2 T-xy diagram 4.3 T-xy diagram ethanol azeotrope 76oc mole fraction of liquid of ethanol 0.425 .1 liquid phase vapor phase 4.4 4.5 .2 80%

%brix refractometer phase %brix dilute ethanol phase %brix phase vapor phase ethanol vapor phase ethanol 90% liquid phase 95% %brix

vapor %brix liquid dilute ethanol 1

azeotrope

azeotrope

5.1

90%

95%

ethanol equilibrium still

60%, 80%,

mole fraction azeotrope ethanol mole fraction of liquid of ethanol 0.425

vapor phase liquid phase T xy diagram 76oc

5.2

% brix liquid phase vapor phase refractometer phase

phase focus %brix

6
1)

azeotrope Ethanol minimum boiling azeotrope ethanol 95.5% 4.5%

78.15

2)

condensate receiver chamber

boiling

Equilibrium
3)

ethanol Ethanol 95 96 %

(azeotrope) Ethanol

concentration 60 % %Brix dilute ( liquid phase) = 5.4 4-1) conc. = 16 % dilute Calibration curve (

C1V1 = C2V2

C1 (1) = ( 16 )(3) C1 = 48 % Basis 100 ml



Ethanol = 48 ml x
     

Water = 52 %

Ethanol = 48 ml x Water = 52 ml x mol fraction , x =



= 0.902 mol

= 2.889 mol

= 0.238 Calibration curve ( 4-1)

%Brix dilute ( vapor phase) = 7.8 conc. = 22.5 % dilute

C1V1 = C2V2

C1 (1) = ( 22.5 )(3) C1 = 67.5 % Basis 100 ml Ethanol = 67.5 ml



Water = 29.5 %

Ethanol = 67.5 ml x Water = 29.5 ml x mol fraction , x =

 

x
  

  

= 1.324 mol

x


= 1.639 mol

= 0.447

. Refractometer Refractometers

(crystal)

( Refraction)

( refraction) Refractometers refractometers ) ) Brix (%) ( water solution) soluble solid) (

( (

Brix (%) (calibration) (cane sugar solution ) 100 Brix (%)

Refractometer

1. Eyepiece refraction field scale

2. Specimen illuminator assembly secondary prism 3. Prism open-shut handles handle secondary 4. Secondary prism Prism secondary prism main prism secondary prism 0.2 main prism prism prism 1 handles

5. Main prism Main prism

main prism 6. Thermistor head Thermistor main prism 7. Scale field of vision illuminator assembly 8. Dessicant case cobalt chloride main prism

9. Temperature control water inlet-outlet nozzles prism 10. Scale adjustment screw 11. Color compensator knob 12. Measurement knob 13.Thermometer

Refractometer Brix (%) Scale

Brix ( water solution) soluble solid)

(%) (

Brix

(%) (cane

sugar

(calibration) solution ) 100 Brix (%)

Fractometer 1. Refractometer Refractometer %Brix 2. Refractometer %Brix

3.